SH/T 0022-1990 Determination of hydrogen content in petroleum fractions (lamp method)

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Card type: Test method

1. Method number / full name / English name / replacement relationship

• Standard number: SH/T 0022-90 (confirmed in 2000)
• Chinese name: Determination of hydrogen content in petroleum fractions (lamp method)
• English name: not provided in the available source
• Replacement relationship: not provided in the available source
• Reference adoption: ASTM D1018-87 "Standard Test Method for Hydrogen Content of Petroleum Fractions"
• Custodianship: Technical custodianship by the Research Institute of Petroleum Processing
• Drafting: Drafted under the responsibility of the Research Institute of Petroleum Processing; main drafter Yang Zhenjie
• Approval/implementation: approved by China Petrochemical Corporation 1991-03-27, implemented on 1992-04-01

2. Scope of application and non-applicability

• Applicable to gasoline, jet fuel, and light diesel fraction.
• Not applicable: not provided in the available source.

3. Method principle

In pure air, the sample is burned through a cotton wick lamp, then the water formed is absorbed from the combustion products with a desiccant, and its hydrogen content is calculated.

4. Reagents and materials (purity / preparation)

4.1 Reagents

• 5.1 Sulfuric acid: chemically pure.
• 5.2 Anhydrous calcium chloride: chemically pure.
• 5.3 Phosphorus pentoxide: chemically pure. Note: phosphorus pentoxide is extremely corrosive; rubber gloves must be worn during operation.
• 5.4 Petroleum ether: analytical reagent, boiling range requires confirmation against the source standard (source-text extraction) (the source text reads "[unreadable characters]901 c", suspected to be a boiling range, requires confirmation against the source standard (source-text extraction)).

4.2 Materials

• 4.2.1 Glass wool.
• 4.2.2 Cotton wick: clean and uniform two-strand twisted cotton wick (new and old cotton wicks must be washed with petroleum ether and dried before use). The mass of each strand of wick is 0.5～0.6 g/m.
• 4.2.3 Gauze and silk cloth.
• 4.2.4 Compressed air. Note: if a compressed air cylinder is used in the test, the regulations for the use of high-pressure gas cylinders must be followed during operation.

5. Apparatus and equipment

• 4.1.1 Lamp: composed of a 25 mL lamp bottle, burner, and lamp cover. The burner is composed of two concentric glass tubes, with a side tube on the outside, and a small hole at the bottom of the burner to balance the pressure between the flue and the lamp bottle. The lamp bottle, burner, lamp cover, and flue are connected to each other with a standard ground joint No. 14. Dimensions are shown in Figure 1.
• 4.1.2 Flue: dimensions are shown in Figure 2.
• 4.1.3 Absorber: dimensions are shown in Figure 3.
• 4.1.4 Air purification system:
  • a. Gas washing bottle: 250 mL;
  • b. Drying tower: 250 mL;
  • c. Conical chamber: filled internally with glass wool. Dimensions are shown in Figure 4;
  • d. Suction flask: serves as a buffer.
• 4.1.5 U-shaped drying tube: filled with anhydrous calcium chloride.
• 4.1.6 Ice-water bath: the volume must be able to accommodate four absorbers (two in series in two rows).
• 4.1.7 Air rotameter: flow range 2～10 L/min (the source text reads "2[unreadable separator]1OL/nuno", requires confirmation against the source standard (source-text extraction)).
• 4.1.8 Balance: sensitivity 1 mg (the source text reads "sensitivity li ngo", requires confirmation against the source standard (source-text extraction)).
• 4.1.9 Desiccator.
• 4.1.10 Pipette: 5 mL.
• 4.1.11 Spring support.
• 4.1.12 Alcohol lamp.

6. Recommended operating conditions

• Air flow rate: during purification system 2～3 L/min; purification system 15 min.
• Amount of sample burned: stop air input at 2～3 g.
• Immersion depth of absorber in ice-water bath is about 5 cm.
• Before weighing, place the desiccator in the balance room for 30 min (or longer).
• Weighing accuracy: weigh to the nearest 1 mg.
• Absorber absorption capacity: one absorber can absorb about 10 g water; when about 10 g water has been absorbed, the desiccant must be replaced.
• Flame requirements: it must be ensured that the flame is steady and symmetrical, with no jetting from the inner cone and no smoke at the outer edge.
• Relationship between wick and sample volatility (Note): the combustion characteristics of the flame are related to the air flow entering the burner, the volatility of the sample, the tightness of the wick in the burner tube, and the position of the wick relative to the burner; the latter two factors can be determined before the experiment. Therefore, during the experiment, the combustion characteristics of the flame are controlled only by adjusting the air flow. For highly volatile samples, the wick is required to be fixed tightly, and the wick is pulled down a few millimeters from the top of the burner tube; for more volatile samples, during combustion, the sample bottle should be immersed in an ice-water bath; for low-volatility samples, the wick is required to be fixed more loosely, and sometimes the sample bottle needs to be heated to ensure that the sample flows steadily into the burner.

7. Sampling and sample preparation

• Reference GB/T 4756 Standard Practice for Manual Sampling of Petroleum Liquids.
• Sample preparation: not provided in the available source.

8. Analytical procedure

8.1 Preparatory work

• 6.1 Packing the absorber: first pack 1～2 cm thick glass wool in sequence; then pack anhydrous calcium chloride 5 cm high, with a particle diameter of about 6～10 mesh; then pack 1 cm thick glass wool; 2 cm thick phosphorus pentoxide; finally, pack glass wool to the top of the absorber. Apply grease to the ground stopper, cover tightly, close the absorber outlet tube, and seal the absorber inlet tube with a rubber tube plug.
• 6.2 Packing the drying tower: pack a small amount of glass wool at the bottom, then pack anhydrous calcium chloride to one-half of the drying tower, with anhydrous calcium chloride particles about 6～10 mesh; add about 1 cm thick glass wool; pack phosphorus pentoxide to the top of the tower, and cover it with a small amount of glass wool.
• 6.3 Pour 100～150 mL sulfuric acid into the gas washing bottle.
• 6.4 Fill the conical chamber with glass wool.
• 6.5 Thread a suitable number of strands of wick through the burner. Draw the wick out through the burner tube with a metal wire. Trim the wick so that it closes the top of the burner as much as possible, and pull the trimmed wick downward so that it is flush with or slightly lower than the burner.

8.2 Test procedure

• 7.1 Assemble the apparatus as shown in Figure 5. Remove the rubber plug of the absorber, connect the two prepared absorbers to each other with a 2 cm short rubber tube, and connect them to the flue. Immerse the lower end of the absorber in an ice-water bath to a depth of about 5 cm.
• 7.2 Connect the clean, dry, assembled lamp (with no sample in the lamp) to the flue.
• 7.3 Connect the air system to the burner side tube, and connect the U-shaped tube to the outlet tube of the second absorber.
• 7.4 Set the valves of the absorber, U-shaped drying tube, and drying tower to the "open" position.
• 7.5 Open the air regulating valve, adjust the air flow rate to 2～3 L/min, and purify the system for 15 min. Close the air regulating valve, close the absorber, and seal the absorber inlet tube with a rubber plug. Remove the absorber from the system. Wipe each absorber clean with clean dry gauze and silk cloth, place it in a desiccator, and place the desiccator in the balance room for 30 min (or longer) so that the absorber reaches room temperature. Before weighing, open the absorber outlet tube, momentarily equalize the pressure, then weigh to the nearest 1 mg.
• 7.6 Use a pipette to take 5 mL sample, inject it into the lamp bottle, insert the prepared burner into the lamp bottle, cover the burner with the lamp cover, and seal the burner side tube with a rubber plug. Capillary action causes the sample to rise to the top of the wick.
• 7.7 Quickly weigh the assembled lamp to the nearest 1 mg.
• 7.8 Immerse the weighed absorber in an ice-water bath (immersion depth about 5 cm). Remove the rubber plug and connect the absorber to the flue.
• 7.9 Set the valves of the absorber, drying tower, and U-shaped drying tube to the "open" position.
• 7.10 Remove the rubber tube plug and lamp cover from the lamp. Connect the air line to the burner side tube. Light the lamp with an alcohol lamp, and at the same time press the stopwatch and record the time when lighting begins. Quickly adjust the air volume until a steady, smokeless flame is obtained, immediately place the lamp into the flue, and support the lamp in a suitable position with the spring support. Stop the stopwatch. The time elapsed from lighting the lamp to placing the lamp into the flue is taken as the lost combustion time (t), and at the same time record the time when the lamp is placed into the flue as the start time of "completion of analysis". After the lamp is placed into the flue, further adjust the air volume so that there is no jetting from the inner cone of the flame and no smoke at the outer edge.
• 7.11 When the sample has burned for 2～3 g, stop the air input, record the time of extinguishing the lamp as the end time of "completion of analysis". Remove the lamp from the system, cover the burner with the lamp cover, and seal the burner side tube with a rubber tube plug. The time elapsed between placing the lamp into the flue and extinguishing the lamp is taken as the "completion of analysis" time (T).
• 7.12 Quickly connect the clean, dry, assembled lamp (with no sample in the lamp bottle) to the flue.
• 7.13 Connect the air system to the burner side tube, and use the air purification system for 5 min (the source text reads "5rr dn", requires confirmation against the source standard (source-text extraction)), with an air flow rate of about 2～3 L/min. If there is condensed water in the flue tube, gently heat the flue tube with an alcohol lamp until all condensed water is evaporated and blown into the absorber, then stop the air input. Remove the absorber, close the absorber outlet tube, seal the inlet tube with a rubber tube plug, wipe clean with dry gauze and silk cloth, and place in a desiccator. Place the desiccator in the balance room for 30 min (or longer) so that the absorber reaches room temperature.
• 7.14 Weigh the mass of the lamp after combustion to the nearest 1 mg. The difference between the mass of the lamp containing the sample before and after the test is the mass of the burned sample (m₂).
• 7.15 After the absorber has been placed in the balance room for 30 min (or longer), weigh it. Before weighing, open the absorber outlet tube, momentarily equalize the pressure, then weigh to the nearest 1 mg. The difference between the mass of the two absorbers in series after the test and before the test is the mass of water formed by burning the sample (m₁).

9. Qualitative and quantitative determination and calculation formula

9.1 Corrected mass of water formed by burning the sample m(g) is calculated according to formula (1):

m = m₁ × T / (T - t)

Where:

• m₁ —— mass of water formed by burning the sample, g;
• T —— completion of analysis time, s;
• t —— lost combustion time, s.

The water generated during the loss of combustion time is not absorbed by the absorber, and therefore needs to be corrected.

9.2 Hydrogen content of the sample X[%(m/m)] is calculated according to formula (2):

X = m × 11.191 / m₂

Where:

• m — the corrected mass of water generated by burning the sample, g;
• m₂ — the mass of the burned sample, g;
• 11.191 — hydrogen content in water, %(m/m).

10. Precision

The reliability of the test results is judged according to the following provisions (95% confidence level).

• 9.1 Repeatability: the difference between two results of repeated determinations by the same operator shall not exceed the value in the table below.
• 9.2 Reproducibility: the difference between two results submitted by different laboratories shall not exceed the value in the table below.

Precision table:

Note: In the original precision table source-text extraction, only “II~ 16 / 0.18” is seen, suspected to be “11～16” and repeatability “0.18”; the reproducibility value is not provided in the available source and requires confirmation against the source standard (source-text extraction).

11. Report

not provided in the available source.

12. Normative references

• GB/T 4756 Petroleum liquids — Manual sampling
• ASTM D1018-87 “Standard Test Method for Hydrogen Content of Petroleum Distillates” (referenced adoption)

13. Source and verification

This page is an AI translation of the available Chinese method card. Human verification is pending. It is not an official translation of the standard. Check the source standard and product certificate before use.

14. Quick Q&A reference